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Sodium Hydroxide → 4-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol

HRID 269899
ノート
印刷プレビュー

反応式

HRID 269899 の反応式
Cl.[CH:2]1([CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]3[CH:22]=[CH:21][C:20]([OH:23])=[C:19]([F:24])[CH:18]=3)[CH2:13][CH2:12]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.C(=O)([O-])O.[Na+].[OH-].[Na+]>C(OCC)(=O)C>[CH:2]1([CH2:8][CH2:9][CH2:10][N:11]2[CH2:16][CH2:15][N:14]([C:17]3[CH:22]=[CH:21][C:20]([OH:23])=[C:19]([F:24])[CH:18]=3)[CH2:13][CH2:12]2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 231114144-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol hydrochloride

生成物 1

HCID 231114094-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol収率 69.9%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

4-[4-(3-Cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol hydrochloride (1.45 g) was suspended in ethyl acetate, and to which saturated aqueous sodium hydrogencarbonate solution and 2 grains of sodium hydroxide were added by the order stated, to effect distribution. The ethyl acetate layer was washed with saturated saline solution, dried over anhydrous magnesium sulfate, and the solvent was distilled off. Purifying the resulting crude product on silica gel column chromatography (eluent, chloroform: methanol=10:1), 4-[4-(3-cyclohexylpropyl)piperazin-1-yl]-2-fluorophenol (910 mg) was obtained.

後処理

  1. washThe ethyl acetate layer was washed with saturated saline solution
  2. dry with materialdried over anhydrous magnesium sulfate
  3. distillationthe solvent was distilled off
  4. customPurifying the resulting crude product on silica gel column chromatography (eluent, chloroform: methanol=10:1)

出典と根拠

ORDレコード
ord-853df0823b0b46e4a000ae41f5b8f83d
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07449466B2

反応ノート

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